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Method for preparing vanadium dioxide low-temperature thermochromic film

A technology of vanadium dioxide and color-changing thin film, applied in ion implantation plating, metal material coating process, coating, etc., can solve the problem of high phase transition temperature, small adjustment range of infrared light, and no visible light transmittance And infrared light adjustment range and other issues, to achieve the effect of reducing the phase transition temperature

Active Publication Date: 2015-07-29
GLASS TECH RES INST OF SHAHE CITY OF HEBEI PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still three serious defects in its specific application: (1) the transmittance of visible light is not high; (2) the adjustment range of infrared light is not large; (3) the phase transition temperature is much higher than room temperature
Thus, the rutile titanium dioxide substrates with different crystal orientations can change the phase transition temperature of vanadium dioxide, and can reduce the phase transition temperature of vanadium dioxide to around room temperature, but the rutile phase titanium dioxide preparation process conditions are harsh (at least 700 ℃ high temperature), high production cost, low practical application value, not suitable for large-scale promotion
[0005] Doping vanadium dioxide with elements such as tungsten can reduce its phase transition temperature to about room temperature, but it will also significantly reduce the visible light transmittance and seriously affect the infrared adjustment ability.
[0006] Chinese patent application number 201210412982.6 discloses a low phase transition temperature vanadium dioxide film preparation process, which directly sputters vanadium dioxide on K9 glass, silicon wafers or other substrates. The patent does not give visible light transmittance and infrared Light adjustment range and other parameters
In addition, for vanadium dioxide grown directly on K9 glass or soda-lime-silica glass, after 400-600 high-temperature tempering and annealing treatment, because there is no sodium ion barrier layer, sodium ions in the glass diffuse into vanadium dioxide to form new compounds , affecting the crystallization of vanadium dioxide, which is not conducive to improving the phase transition characteristics of vanadium dioxide

Method used

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Embodiment 1

[0033] Using DC reactive magnetron sputtering technology, high-purity metal vanadium is used as the target material, glass is used as the substrate, high-purity oxygen and argon are used as the reaction gas and sputtering gas, and the background vacuum is pumped to 1-3x10 -4 Pa, then feed a certain amount of oxygen and argon, so that the oxygen partial pressure is 10%, the working pressure is 1.0Pa, the substrate temperature is room temperature, and a 100nm thick vanadium pentoxide film is grown, and then the temperature is raised to 400°C. The oxygen / argon gas is 45%, the working pressure is 0.8Pa, and high-purity metal titanium is used as the target material to induce sputtering growth of 150nm rutile titanium dioxide film. Through a solid-liquid reaction mechanism, the substrate / rutile titanium dioxide / vanadium pentoxide structure was realized, followed by annealing at 400 °C for 1 hour in a reducing atmosphere. The SEM images of the obtained samples are shown in figure 1 ...

Embodiment 2

[0035] Using DC reactive magnetron sputtering technology, high-purity metal vanadium is used as the target material, glass is used as the substrate, high-purity oxygen and argon are used as the reaction gas and sputtering gas, and the background vacuum is pumped to 1-3x10 -4 Pa, feed a certain amount of oxygen gas and argon gas then, the oxygen / argon gas flow ratio that makes is 30%, working pressure is 1.0Pa, and substrate temperature is room temperature, grows the thick vanadium pentoxide thin film of 120nm, then heats up to 400°C, oxygen / argon 40%, working pressure 0.2Pa, high-purity titanium metal as target, power density 4.5W / cm2, induced sputtering growth rutile titanium dioxide film 150nm. Through a solid-liquid reaction mechanism, the substrate / rutile titania / vanadium pentoxide structure is realized, and then the N 2 Anneal at 700°C for 1 hour in an inert environment. The SEM images of the obtained samples are shown in figure 2 As shown, the phase transition tempera...

Embodiment 3

[0037] Using DC reactive magnetron sputtering technology, high-purity metal vanadium is used as the target material, glass is used as the substrate, high-purity oxygen and argon are used as the reaction gas and sputtering gas, and the background vacuum is pumped to 1-3x 10 -4Pa, then feed a certain amount of oxygen and argon, so that the oxygen / argon flow ratio is 20%, the working pressure is 0.5Pa, the substrate temperature is 200°C, grow a 100nm thick vanadium pentoxide film, and then heat up To 400°C, the oxygen / argon gas is 12%, the working pressure is 0.2Pa, high-purity metal titanium is used as the target, the power density is 5W / cm2, and the rutile titanium dioxide film is grown by sputtering to 150nm. Through a solid-liquid reaction mechanism, the substrate / rutile titanium dioxide / vanadium pentoxide structure was realized, followed by annealing at 400 °C for 1 hour in a reducing atmosphere. The phase transition temperature of the vanadium dioxide thin film is 38°C.

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Abstract

The invention discloses a method for preparing a vanadium dioxide low-temperature thermochromic film. The method comprises the steps of cleaning and loading a substrate, then, depositing a vanadium pentoxide layer as an inducing layer in advance, then, growing a mixed-crystal-orientation rutile titanium dioxide buffer layer on the vanadium pentoxide layer through solid-liquid induction, moving vanadium pentoxide of the bottom layer to the top layer after induced growth so as to form a crystalline rutile-phase titanium dioxide and vanadium pentoxide mixed film, and reducing vanadium pentoxide of the top layer into vanadium dioxide through a reducing atmosphere, thereby finally obtaining a substrate / rutile titanium dioxide / rutile vanadium dioxide thermochromic film. According to the obtained film, the phase change temperature is close to room temperature, and the film has sufficient visible light transmission rate and infrared switching efficiency, so that the needs of occasions, such as building intelligent windows and automotive glass, on practical application can be met.

Description

technical field [0001] The invention relates to a method for preparing a low-temperature thermochromic film of vanadium dioxide, which belongs to the technical field of functional materials and films, and specifically relates to the use of vanadium pentoxide to induce sputtering at low temperature to grow rutile titanium dioxide with a specific crystal orientation, and to reduce it on the substrate A method for preparing vanadium dioxide low-temperature thermochromic film from vanadium pentoxide in the upper layer. Background technique [0002] Vanadium dioxide is a phase change material. Its M phase and R phase will change from an infrared transparent semiconductor phase (M) to an infrared opaque metal phase (R phase) at 68 ° C, accompanied by optical, electrical and magnetic properties. The sudden change in performance, these characteristic changes can be used in smart windows, thermal sensitive resistors, satellite lens laser protection, temperature control switches, opti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/35C23C14/08C23C14/58
Inventor 陈支勇潘清涛栾晓波程金树袁坚王芮秦伟
Owner GLASS TECH RES INST OF SHAHE CITY OF HEBEI PROVINCE
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